In vitro Mechanical Testing of Glass Fiber-reinforced Composite Used as Dental Implants Abstract Aim: The aim of this study was to evaluate the design of fiber-reinforced composite (FRC) on some mechanical properties of a dental implant. Methods and Materials: FRC implants were fabricated using different polymerization conditions and designs of the glass-fiber structure. Specimens were tested with a cantilever bending test and a torsional test. The degree of monomer conversion (DC%) was measured using a Fourier transform infrared spectroscopy (FTIR). Results: Statistical analysis showed significant differences between groups revealing mean fracture load values from 437 N to 1461 N. The mean torsional force in fracture varied from 0.01 to 1.66 Nm. The DC% varied from 50% to 90%. Conclusion: This study suggests by modifying the polymerization conditions and fiber orientation of FRC implants, the biomechanical properties of an FRC can be tailored to the needs of dental implants. Keywords: Dental implant, fiber-reinforced composite, FRC, mechanical properties, bending overload, torsion load, failure force Citation: Ballo AM, Lassila LV, Närhi TO, Vallittu PK. In vitro o Mechanical Testing of Glass Fiber-reinforced Composite Used as Dental Implants. J Contemp Dent Pract 2008 February;(9)2:041-048. © Seer Publishing 1 The Journal of Contemporary Dental Practice, Volume 9, No. 2, February 1, 2008 Introduction Dental implant treatment is one of the commonly used conservative methods of permanently replacing one or more missing teeth.1 Dental implants have traditionally been made of metal. The use of pure titanium or a titanium alloy has been the material of choice. Occasionally complications during the first year of functional loading occur, but the most common complications are loosening of abutments or bridge screws and esthetics related.2 Functional occlusal load and overloading of dental implants during mastication has been extensively studied and discussed,3,4 but less work has been done on torsional loading forces of the implants.5 In an oral environment dental implants are subjected 4,6,7 to multidirectional forces. Forces can have either vertical or horizontal components, but also 4 inclined and torsional forces may exist. The bending moment due to forces deviating from the direction of the implant axis can produce higher stress in the implant and implant-bone interface than a direct axial load.4,8 The magnitude of occlusal forces varies depending on tooth position in the mouth.4 The mean maximal occlusal forces in the incisal area have been reported to range from 264 N to 370 N11,12 whereas the maximum biting force in the posterior area can be around 800 N.13 Fiber reinforced composites (FRC) are a relatively new group of materials investigated in dental or medical applications over the last 30 years.14 Their use is growing in many dental applications including use in implant-supported prostheses.15-17 In the FRC the fibers are made of E-glass or quartz and are translucent which provides for 18 favorable esthetics. Microbial adhesion to FRC has been shown to be lower in glass FRC 19 than in a FRC made of polyethylene fibers. Furthermore, an FRC implant is relatively easy to grind and modify directly in the mouth in order to properly restore the implant abutment area with composite superstructures without having a risk of overheating underlying bone. Proper treatment planning for implant placement and careful crown fabrication with optimal cusp inclination can normally prevent implant overload.9 The excessive bending moments may cause stress concentration and micro-fractures in alveolar bone and even implant fractures. Mechanical properties of FRCs are well documented by many investigators.20,21 The optimal mechanical properties for FRC in bending can be obtained with continuous unidirectional fibers.22 The modulus of elasticity of FRC (20-40 GPa) varies according to fiber volume and can be tailored to simulate stiffness close to natural bone.23 In addition, a mismatch of the modulus of elasticity of the bone and the high stiffness metallic implant induces the stress-shielding effect, which means the implant does not strain and load the bone physiologically similarly as the absence of the implant. This causes loss of 10 bone and bone contact. For this reason, the concept of using a material with similar modulus of elasticity to bone has become an issue of interest. By lowering the modulus of elasticity, the mechanical properties of the implant can better match the properties of bone which further provides mechanical stimulus to the bone. Effective wetting of fibers by the resin matrix, also referred to as resin impregnation, is a pre-requisite for their effective use.20,24 In the case of photopolymerization of FRC, the light intensity, exposure time, and the polymerization temperature has an effect on flexural properties 25 and monomer conversion. Effects of water sorption on the flexural properties of FRCs have also been reported.26,27 Recently, attempts have been made to use FRC as implant material in head and neck surgery.28 Our previous study 2 The Journal of Contemporary Dental Practice, Volume 9, No. 2, February 1, 2008 showed preosteoblasts can mature and proliferate well on the FRC substrates giving support to the use of FRC in a bone environment.29 prepare the specimens. The size of specimens was based on the assumption if they were to be used as oral implants their load-bearing capacity should exceed average maximum occlusal forces within the physiological strain limit of bone.33 The fibers were inserted into the mold along the long axis of the specimens. Both continuous unidirectional resin preimpregnated (prepregs) and manually impregnated resin fibers were used (Table 2). The resin system was a dimethacrylate-monomethacrylate (BisGMA-PMMA) system that produced a semiinterpenetrating polymer network to form a polymer matrix. Bioactive glass (BAG) implant coatings have been shown to improve osseointegration both in in vitro o and in vivo o conditions.30,31 BAG particles may be used as a bioactive component in FRC devices since they can be embedded within the resin matrix or applied on the surface of the FRC implants which may improve osseointegration. The aim of this in vitro o study was to evaluate bending and torsion properties and degree of monomer conversion (DC%) of FRC implant shaped test specimens in order to determine their suitability as a potential implant material. Experimental materials and polymerization conditions of the specimens are summarized in Table 2. Six groups of specimens were prepared with eight specimens fabricated for each group. Various polymerization conditions were tested for optimizing the polymerization of the resin matrix. The test specimens were polymerized with an Optilux 501 hand light-curing unit (Kerr Mfg., Orange, CA, USA), in a light curing oven at 80°C (LicuLite, Dentsply De Trey GmbH, Dreieich, Germany) and post-cured at 120°C which was the temperature of glass transition (Tg) of the pBisGMA-pTEGDMA-copolymer. Methods and Materials The materials used for the fabrication of the specimens for bending and torsion tests are listed in Table 1. Each specimen contained seven fiber reinforcements each of them consisting of 4000 single glass fibers of 15 μm in diameter. The E-glass fiber composition was: 55% SiO2, 15% Al2O3, 22% CaO, 6% B2O3 and 0.5% MgO, >1.0% Fe +Na + K. The modulus of elasticity of FRC material is mostly affected by the volume of fiber and the degree of conversion of the polymer matrix.32 In this unidirectional FRC the modulus of elasticity is between 20 and 40 GPa. After polymerization, the specimens were wet ground with 1200 grit (FEPA) silicon carbide grinding paper after which the diameter and length of the specimens were measured at three different places in order to record the final dimensions of the specimens. The specimens were conditioned in air at room temperature for two days before mechanical testing. Specimen Preparation Molds with an internal diameter of 4 mm and length of 20 mm and 30 mm were used to Table 1. Materials used in the study. *Bis-GMA, bisphenol A-glycidyl dimethacrylate. **TEGDMA, triethylenglycoldimethacrylate. ***PMMA, poly methyl methacrylate, Mw 220.000 **** E-glass, electrical glass 3 The Journal of Contemporary Dental Practice, Volume 9, No. 2, February 1, 2008 Table 2. Classification of experimental FRC specimens used in this study according to the polymerization conditions and design of fiber reinforcement. Note: everStick™ was used in the fabrication of PMMA specimens in groups A, B, C, D, and E whereas in group F the reinforcement was done using continuous unidirectional E-glass with manual bisGMA-TEGDMA resin impregnation (Stick Resin, StickTech). * see Figure 6. Specimen Testing For the cantilever bending test, 10 mm of each specimen (4 mm diameter and 20 mm long) was embedded from one end into the center of a 10 mm x 10 mm x 10 mm acrylic resin block. The cantilever bending test was performed to measure the flexural properties of the specimens. A jig was used to provide a 45° angle between the long axis of the implant and the direction of the loading force (Figure 1). The specimens were loaded to failure using a Lloyd Model LRX material testing machine (Lloyd Instruments Ltd., Fareham, England) with acrosshead speed of 1.0 mm/min until fracture. Fracture force was determined as an audible crack or 10% reduction in force indicated by the testing device. The peak force of the failure of each specimen was recorded with Nexygen PC software (Lloyd Instruments Ltd., Fareham, England). Figure 1. Cantilever bending test of the specimen. into the center of a 10 mm x 10 mm x 10 mm acrylic resin block. Specimens were tested for the resistance of torsional force to failure using the same Lloyd Model LRX universal testing machine but with an angle speed of 16.2 degrees/min. A TP-2KMCB torsion sensor (KYOWA Machine Ltd., Tokyo, Japan) was used to measure maximum torsional force of the specimen (Figure 2). Failure types of test specimens after the bending test were visually classified to the following groups: A. Delamination of the prepregs. B. Fracture of the test specimen. C. Delamination of the fiber weaves from the core. D. For the torsional force test, 10 mm of each cylindrical specimen, 4 mm diameter and 30 mm long, were embedded from both ends SEM micrographs illustrate the delamination of prepregs and fiber weaves (Figures 3 and 4). 4 The Journal of Contemporary Dental Practice, Volume 9, No. 2, February 1, 2008 The DC% of the polymer matrix of mechanically tested specimens after various polymerization modes was monitored using Fourier transform infrared spectroscopy (FTIR) (Spectrum One, Perkin Elmer, Beaconsfield Bucks, UK) with an attenuated total reflectance (ATR) sampling accessory. The mechanically tested specimens were ground with a grinding stone to collect powder to be placed on the surface of the detector ZnSe-ATR crystal of the FTIR spectroscope. The spectrum of unpolymerized resin matrix of the everStick reinforcement (Stick Tech Ltd, Turku, Finland) was used to measure the DC% of polymer powder of each specimen. Each spectrum was recorded with 16 scans using a resolution of 4 cm. The DC% was calculated from the aliphatic C=C peak at 1638 cm and normalized against the aromatic C=C peak at 1608 cm according to following formula: Figure 2. Schematic diagram of torsional loading test of the specimen. Where: Caliphatic = absorption peak at 1638 cm−1 of the cured specimen Caromatic = absorption peak at 1608 cm−1 of the cured specimen Ualiphatic = absorption peak at 1638 cm−1 of the uncured specimen Uaromatic = absorption peak at 1608 cm−1 of the uncured specimen Figure 3. SEM micrographs illustrate the delamination of the prepregs. Data Analysis Data were analyzed statistically with analysis of variance (ANOVA) (SPSS, SPSS Inc., Chicago, IL, USA) followed by a Tukey’s post hoc analysis using a significance level of p<0.05. Results Tables 3 and 4 illustrate the mean fracture load values and standard deviations for the specimens. The ANOVA revealed post-curing significantly affected the fracture load (p<0.001). The mean fracture load values were: 437 N for group A, 581 N for group B, 961 N for group C, 1108 N for group D, 1461 N for group E, and 1200 N for group F. The torque could not be determined for the specimens in groups A, B, C, and D because of delamination of FRC prepregs in the early stage of loading. The mean torque Figure 4. SEM micrographs illustrate fracture and delamination of the fiber weaves. 5 The Journal of Contemporary Dental Practice, Volume 9, No. 2, February 1, 2008 Table 3. The mean failure load values and standard deviation of the test specimens in cantilever bending test (n=8). Same superscript letter indicates groups did not differ statistically significantly (p<0.05). Table 4. The mean maximal torsional force and standard deviation of the test specimens (n=8). Same superscript letter indicates groups did not differ statistically significantly (p<0.05). Table 5. The degree of conversion (DC%) and standard deviation of polymer matrix of tested specimens after different polymerization conditions. Same superscript letter indicates groups did not differ statistically significantly (p<0.05). was 1.66 Nm (range 1.3 to 1.9 Nm) for group E and 1.0 Nm (range 0.8 to 1.4 Nm) for group F. Three types of failure patterns were found (Figure 5). Failure pattern A was found in groups A-D specimens, B in group E, and C in group F. The DC% is presented in Table 5. The mean DC% increased in all groups by increasing the time of light curing and by increasing the postcuring temperature. The specimens in group A had the lowest DC%; the mean DC% was 53% for group A, 61% for group B, 73% for group C, 75% for group D, and 90% for group E and F. Discussion The mechanical link between a natural tooth and the surrounding bone is provided by the periodontal ligament (PDL) which controls the dynamics of the tooth under load. By comparison, a dental implant is integrated to the 6 The Journal of Contemporary Dental Practice, Volume 9, No. 2, February 1, 2008 Figure 5. Schematic diagram of failure patterns of test specimens after cantilever bending test in Group A-F: A. Delamination of the prepregs. B. Fracture of the test specimens. C. Delamination of the fiber weaves from the core. Table 6. Comparison of mechanical properties of different implant materials. bone without a PDL. The mismatch of stiffness between bone and implant material can lead to implant failures especially in conditions where either bone quantity or quality is poor. This can occur if the tensile or compressive load exceeds the physiological limit of bone tolerance and causes microfracture at the bone-to-implant interface or initiates bone resorption. On the other hand, implant material that is too stiff does not provide the normal physiological stimulus on bone which causes loss of bone around the implant. dental implant material. Recently, Zirconia has been introduced as a new ceramic dental implant material, but has a stiffness (modulus 200 GPa) that is too high compared to bone. It also has a very high modulus of elasticity (17–24 GPa) compared to human bone. As a metal substitute, Zirconia possesses good chemical and physical properties, like low corrosion potential and low thermal conductivity.39-41 Furthermore, its biocompatibility and biomechanical properties as dental implant 42-44 material has been extensively investigated. Different materials have been introduced for the construction of dental implants. Table 6 illustrates 34,35 the mechanical properties of these materials. The pure titanium (Ti) and Ti alloy offer favorable physical properties. Ti offers many of the desirable attributes for an implant material such as excellent inertness, resistant to corrosion by body fluids, and apparent compatibility with living tissue.1,36,37 Hydroxyapatite (HA) ceramic has been investigated extensively and used for dental implant applications for the past 30 years. HA properties depend on its porosity. Clinical studies demonstrated HA ceramics still remain the most biocompatible bone implant material known and possess the added benefit of strong bonding to living bone through natural-appearing bonding mechanisms,45 but they can fracture during surgery and after loading.46 Therefore, HA ceramics are not ideal materials for permanent implant devices. However, bioactive ceramic coatings on metal implants has helped to retain ceramics as a key component in dental 47,48 implantology. Ceramic material like aluminum oxide (Al2O3) 38 has been utilized as a dental implant material. This material has osseointegrated favorably, but unfortunately the biomechanical properties (modulus 300GPa) of the implants were not sufficient for a long-term load. As a result, this material has been withdrawn from the market as 7 The Journal of Contemporary Dental Practice, Volume 9, No. 2, February 1, 2008 DC% level. However, further studies are needed to determine the surface characteristics required for optimizing the bonding of FRC to bone by using such strategies as bioactive ceramic coatings on FRC implants. FRC are durable materials with good flexural properties because it has a lower elastic modulus than metals.22,49 In fact, the mechanical properties and modulus of elasticity of unidirectional FRC (20-40 GPa) are close to natural bone. The FRC structure makes it possible to embed bioactive ceramic particles (such as BAG) within the resin matrix or apply them directly to the surface of FRC implants. Such an implant structure may be suitable for the clinical applications involving poor bone quality. It is well known higher DC% results in better mechanical properties for the polymer and composite material than lower DC%.57 A higher DC% can be obtained by lengthening the polymerization time and increasing the polymerization temperature. Improvement in mechanical properties by the increased DC% are related to the increased cross-linking density which increases the number of covalent bonds between polymer backbones and lowers the amount of residual monomers that could 58-60 plasticize the polymer matrix. The present study also confirmed this by showing substantial improvement in bending and torsional properties of the specimens with a high DC%. A three times higher load to failure ratio of implant specimens was observed in group D compared to group A. The quantity of leachable residual monomers decreases with an increasing DC%. Thus, in addition to improved strength, a high DC% obviously improves the biocompatibility which is required for implant materials. The most typical application of FRC material in dentistry is on endodontically treated teeth restored with fiber posts. The published information regarding the clinical survival rate failure rate was reported to be 12.8% within a 24 month observation period after fiber reinforced 50 posts were placed. While another study showed the cumulative failure rate for metal posts was 11.2% within ten years.51 However, the typical difference between metal and FRC posts in cases of failure is metal post causes root fracture whereas failure of FRC post occurs at the crown level leaving the root intact and repairable. This phenomenon can be explained by the mismatch between the high stiffness metal and the dentin, thus, supporting the concept of an FRC implant. The fatigue test showed statistically significant differences among the different posts due to variations in fiber post manufacturing process.52 Commercially available prefabricated FRC posts showed lower flexural properties than an individually polymerized FRC material.53 In groups A-D the failure occurred by producing cracks and delamination of resin prepregs (interfacial failure), followed by a growing crack at the interface between the prepregs. This problem could be overcome by improving the interfacial adhesion of the prepregs used in specimen fabrication or by alternatively using a different fabrication process as was used in groups E and F. This study was conducted to determine some mechanical properties of a metal-free FRC material which could be further evaluated as a potential dental implant material. The test set-up was designed to simulate simple clinical loading conditions of an implant. Specimens in group E and F were prepared to avoid delamination by changing the fabrication process. In group E the specimens were coated with fiber weave to encapsulate the unidirectional fibers together (Figure 6), whereas in group F the specimens were made of manually impregnated fibers as one large sized roving. The four times higher load to failure ratio obtained in group E compared to Group A suggests the fiber weave effectively protected the unidirectional fibers against delamination. The introduction of a new biomaterial for surgical use requires a number of preclinical studies. The materials used in this study were made of pBis-GMA-pTEGDMA copolymer, which is already widely used and generally accepted as 54-56 bone cement. From this perspective, the currently tested resin materials can be estimated to be acceptable for the use in dental implants, especially if they have been polymerized to a high This in vitro o study showed the mean static load to failure ratio of specimens in all groups was 8 The Journal of Contemporary Dental Practice, Volume 9, No. 2, February 1, 2008 torque data was not available for the specimens in groups A-D. Encapsulation of unidirectional FRC with a fiber weave (Group E) improved the resistance to torsion loading. Since this specimen design showed the best mechanical properties in the present study it seems to hold the greatest potential for in vivo o studies. The basic challenge in the manufacture of a FRC implant has been reinforcement of the thread on the screw shape implant design which has been overcome by reinforcing the threads with external bidirectional fiber coating.61 Figure 6. Schematic diagram of test specimen fabricated for group E: continuous unidirectional FRC core (A) was encapsulated with a bidirectional fiber weave (B) (0 +/-90° fiber angle). In a clinical situation FRC implant fractures offer a challenging problem because of functional, restorative, and surgical implications. This complication can be solved by restoring the FRC implant with composite superstructures. above the previously reported maximum incisal biting force. Whereas the mean load of failure for groups D, E, and F were beyond the reported maximum posterior bite force.13 However, flexural fatigue studies are needed to simulate the dynamic loading conditions by the masticatory system. Conclusions Within the limitations of this study it can be concluded: 1. Failure forces of FRC specimens with an average diameter of dental implant exceeded reported maximum static human bite forces. 2. Encapsulation of continuous unidirectional glass fibers with a fiber weave, improves the resistance FRC specimens to torsional and bending forces. 3. Prolonging of polymerization time and increasing the polymerization temperature increases the DC% of the polymer matrix of FRC. Torsional loading produced maximum shear stress and twisted the structure along the neutral axis. Shear stress increases as a function of distance from the neutral axis. With a torsional load, the specimens in groups A, B, C, and D exhibited twisting at the very early moment of loading and delamination occurred before a torsional load was registered. As a result, References 1. Brånemark PI, Hansson BO, Adell R, Breine U, Lindstrom J, Hallen O. Osseointegrated implants in the treatment of the edentulous jaw: experience from a ten year period. Scand J Plast Reconstr Surg Suppl. 1977; 16:130-6. 2. Jemt T, Linden B, Lekholm U. 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Oper Dent. 1994; 19:26–32. 59. Asmussen E, Peutzfeldt A. Mechanical properties of heat treated composite resin inlay/onlay technique. Scand J Dent Res. 1990; 98:564-7. 60. Loza-Herrer MA, Rueggeberg FA. Time temperature profiles of post-cure composite oven. Gen Dent. 1998; 46:79-83. 61. Ballo AM, Lassila LV, Vallittu PK, Närhi TO. Load bearing capacity of bone anchored fiber-reinforced composite device. J Mater Sci-Mater Med. (Accepted for publication). About the Authors 12 The Journal of Contemporary Dental Practice, Volume 9, No. 2, February 1, 2008 Acknowledgement The first author would like to thank the ITI Foundation for providing a research scholarship in support of this investigation. 13 The Journal of Contemporary Dental Practice, Volume 9, No. 2, February 1, 2008
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